Propionaldehyde (crude, 25mL) was distilled in a 100mL round bottom flask under a gentle flow of N2 gas. The distillate was collected as 3 fractions in graduated centrifuge tubes
Log
10:10 Started heating crude propionaldehyde on a heating mantle with variac in a 100ml round single neck round bottom flask under a gentle flow of N2 (one bubble a sec) The crude propionaldehyde was constantly stirred with a mag. stirrer. (Variac (V)-60 Temp (t) 25.
10:22 V-60; t-26
10:23 Reflux started 3 drops a sec.
10:29 V-60, t= 46
10:31 First drop in the fraction collector.
10:40 About 0.7mL (118-F1)distillate collected, changed the fraction collector.
10:40 V-60, t= 45
10:52 Collected about 0.8mL distillate in the fraction collector- 118-F2
10:55 Changed the fraction collector....
11 05 Turned off the variac, stopped heating. Third fraction still plugged in...don't need it
Purification of Propionaldehyde
Objective
To purify propionaldehyde by distillation.Procedure
Propionaldehyde (crude, 25mL) was distilled in a 100mL round bottom flask under a gentle flow of N2 gas. The distillate was collected as 3 fractions in graduated centrifuge tubesResults
PropionaldehydeCrude
HNMR
Fraction-2
HNMR
Conclusion
Distillation was successful.
Log
10:10 Started heating crude propionaldehyde on a heating mantle with variac in a 100ml round single neck round bottom flask under a gentle flow of N2 (one bubble a sec) The crude propionaldehyde was constantly stirred with a mag. stirrer. (Variac (V)-60 Temp (t) 25.
10:22 V-60; t-26
10:23 Reflux started 3 drops a sec.
10:29 V-60, t= 46
10:31 First drop in the fraction collector.
10:40 About 0.7mL (118-F1)distillate collected, changed the fraction collector.
10:40 V-60, t= 45
10:52 Collected about 0.8mL distillate in the fraction collector- 118-F2
10:55 Changed the fraction collector....
11 05 Turned off the variac, stopped heating. Third fraction still plugged in...don't need it
A picture of the setting.